CN106001605B - A kind of method that Fe nano particles are prepared using carbon quantum dot as crystal seed - Google Patents
A kind of method that Fe nano particles are prepared using carbon quantum dot as crystal seed Download PDFInfo
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- CN106001605B CN106001605B CN201610510520.6A CN201610510520A CN106001605B CN 106001605 B CN106001605 B CN 106001605B CN 201610510520 A CN201610510520 A CN 201610510520A CN 106001605 B CN106001605 B CN 106001605B
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention relates to a kind of method that Fe nano particles are prepared using carbon quantum dot as crystal seed, this method comprises the following steps：(1) ferric acetyl acetonade is dissolved in oleyl amine solution, is stirred at room temperature and is passed through inert nitrogen gas heating, insulation, while be rapidly injected tri octyl phosphine at such a temperature；Then heat up, be incubated, obtain dark red liquid；(2) citric acid is added in oleyl amine solution, adds octadecylene and be uniformly mixed, be stirred at room temperature and be passed through inert nitrogen gas heating, insulation, while be rapidly injected tri octyl phosphine；After insulation terminates, faint yellow clarified solution is obtained；(3) the dark red liquid of the step (1) gained will be injected after the faint yellow clarified solution heating, and the protection that injection finishes in inert nitrogen gas drops to room temperature, obtains black liquor；(4) the black liquor produces magnetic metal Fe nano particles through centrifuging, washing, being dried under vacuum to constant weight.The inventive method is simple, cost is relatively low, environmental pollution is small.
Description
Technical field
The present invention relates to the preparing technical field of magnetic Nano material, more particularly to one kind to prepare by crystal seed of carbon quantum dot
The method of Fe nano particles.
Background technology
In recent years, magnetic Nano material is due to electricity, optics, magnetics and excellent chemical property with uniqueness, in core
Magnetic resonance imaging, optical nano device, targeted drug, magnetic storage, catalyst etc. have it to be widely applied, thus prepare single
Disperse, particle diameter is small, even size distribution magnetic nano-particle turns into the focus for studying functional form nano material.Magnetic Nano
The preparation method of particle is generally divided into Physical, chemical method and physical-chemical process, and wherein Physical mainly has mechanical attrition method, magnetic
Control sputtering method etc..It is also higher to equipment requirement because the technological process of these physical methods is complex, come relative to Physical
Say, chemical method has more very big advantage in size, crystal formation and pattern of control particle etc..
The content of the invention
The technical problems to be solved by the invention are to provide that a kind of method is simple, cost is relatively low, environmental pollution is small with carbon
Quantum dot is the method that crystal seed prepares Fe nano particles.
To solve the above problems, a kind of method that Fe nano particles are prepared using carbon quantum dot as crystal seed of the present invention,
Comprise the following steps：
(1) ferric acetyl acetonade is dissolved in oleyl amine solution, is stirred at room temperature and is passed through 10 ~ 40min of nitrogen, then exist
100 ~ 200 DEG C are heated to 5 ~ 20 DEG C/min speed under the protection of nitrogen, and in 10 ~ 60min of insulation at this temperature, while
Tri octyl phosphine is rapidly injected at this temperature；Then temperature is raised to 150 ~ 250 DEG C, and in being incubated 10 ~ 60min at this temperature, obtained
To dark red liquid；The mass volume ratio of the ferric acetyl acetonade and the oleyl amine solution is 0.1 ~ 1.5mmol：5~20mL；Institute
The mass ratio for stating ferric acetyl acetonade and the tri octyl phosphine is 0.1 ~ 1.5mmol：1.00~5.00mmol；
(2) citric acid is added in oleyl amine solution, adds octadecylene and be uniformly mixed, be stirred at room temperature and lead to
Enter 10 ~ 40min of nitrogen, be then heated to 150 ~ 250 DEG C under the protection of nitrogen with 5 ~ 20 DEG C/min speed, and in the temperature
20 ~ 100min of lower insulation, while tri octyl phosphine is rapidly injected at such a temperature；After insulation terminates, faint yellow clarified solution is obtained；Institute
The mass volume ratio for stating citric acid and the oleyl amine solution is 0.01 ~ 0.1g：0.5~5mL；The citric acid and the octadecylene
Mass volume ratio be 0.01 ~ 0.1g：1~10mL；The mass ratio of the citric acid and the tri octyl phosphine is 0.01 ~ 0.1g：
1.00~5.00mmol；
(3) the faint yellow clarified solution is continued to be warming up to 250 ~ 350 DEG C, and at this temperature using syringe pump injection institute
The dark red liquid of step (1) gained is stated, the protection that injection finishes in nitrogen drops to room temperature, obtains black liquor；
(4) the black liquor obtains sediment after centrifugation, and mixed liquor washing 3 of the sediment through n-hexane-ethanol ~
It is 9 times, vacuum dried to constant weight, produce Fe nano particles.
The step (1) ~ (3) the flow velocity of middle nitrogen be 30 ~ 60mL/min.
(3) middle injection rate is 1 ~ 10mL/h to the step.
(4) the volume ratio of the mixed liquor of middle n-hexane-ethanol and black liquor is 0.5 ~ 3 mL to the step：1 mL.
The mixed liquor of the step (4) middle n-hexane-ethanol refers to n-hexane and absolute ethyl alcohol by 2 ~ 4：1 volume ratio
Mix.
The condition of the step (4) middle centrifugation refers to that centrifugation rate is 4000 ~ 9000rpm, and the time is 120 ~ 300 seconds.
The step (4) in vacuum drying condition refer to temperature be 30 ~ 60 DEG C, vacuum be -0.09 ~ -0.07MPa.
The present invention has advantages below compared with prior art：
1st, for the present invention using ferric acetyl acetonade as presoma, oleyl amine and octadecylene be solvent, introducing carbon quantum dot as crystal seed,
Prepare that highly crystalline, purity is high, the Fe nano-particles of the body-centered cubic phase of uniform particle diameter by high temperature organic liquid phase method.
2nd, the addition of quantum dot improves the surface state of Fe nano-particles caused by high temperature organic liquid phase method in the present invention,
Curing beneficial to amorphous Fe crystallizes, so as to obtain the very high product of crystallinity.
3rd, the present invention have chosen nontoxic and higher boiling point oleyl amine and octadecylene as reaction dissolvent, reduce to environment
Pollution.
4th, x-ray diffraction experiment is carried out to Fe nano particles obtained by the present invention, it can be found that 2 θ=(44.673,65.021 Hes
82.333 °) there is diffraction maximum in place, and these diffraction maximums correspond respectively to Fe (110), (200), (211) crystal face (referring to figure
1) the Fe nano-particles for, illustrating to obtain are body-centered cubic phase, and as can be seen from the figure product crystallinity is high, and purity is high.Enter one
Step is tested through SEAD（Referring to Fig. 3）, it can be seen that product crystallinity is very high, consistent with XRD test results.
5th, the Fe nanoparticle sizes that synthesize of the present invention are homogeneous and narrow distribution, good dispersion（Referring to Fig. 2）.
6th, the present invention uses and is continuously injected into method so that product grain is uniform.
7th, the inventive method is simple, cost is relatively low.
Brief description of the drawings
The embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 is the X ray diffracting spectrum (XRD) of Fe nano particles of the present invention.Using D/max-2400 type X-ray diffractions
Instrument, excitation source are the nm of λ=1.5406（Japanese Rigaku companies）.
Fig. 2 is transmission electron microscope (TEM) photo of Fe nano particles of the present invention（100nm）.Using TECNAI G2 TF20 types
Transmission electron microscope（FEI Co. of the U.S.）.
Fig. 3 is the SEAD of Fe nano particles of the present invention（SAED）Photo.It is saturating using TECNAI G2 TF20 types
Penetrate electron microscope（FEI Co. of the U.S.）.
Embodiment
A kind of method that Fe nano particles are prepared using carbon quantum dot as crystal seed of embodiment 1, comprises the following steps：
(1) ferric acetyl acetonade is dissolved in oleyl amine solution, is stirred at room temperature and is passed through nitrogen 10min, then in nitrogen
Protection under with 5 DEG C/min speed be heated to 100 DEG C, and in being incubated 10min, while quick note at such a temperature at this temperature
Enter tri octyl phosphine；Then temperature is raised to 150 DEG C, and in being incubated 10min at this temperature, obtains dark red liquid.
Wherein：The mass volume ratio of ferric acetyl acetonade and oleyl amine solution is 0.1mmol：5mL；Ferric acetyl acetonade and trioctylphosphine
The mass ratio of phosphine is 0.1mmol：1.00mmol.
(2) citric acid is added in oleyl amine solution, adds octadecylene and be uniformly mixed, be stirred at room temperature and lead to
Enter nitrogen 10min, be then heated to 150 DEG C under the protection of nitrogen with 5 DEG C/min speed, and in being incubated at this temperature
20min, while tri octyl phosphine is rapidly injected at such a temperature；After insulation terminates, faint yellow clarified solution is obtained.
Wherein：The mass volume ratio of citric acid and oleyl amine solution is 0.01g：0.5mL；The mass body of citric acid and octadecylene
Product ratio is 0.01g：1mL；The mass ratio of citric acid and tri octyl phosphine is 0.01g：1.00mmol.
(3) faint yellow clarified solution is continued to be warming up to 250 DEG C, and at this temperature using syringe pump with 1mL/h speed note
Enter the dark red liquid of step (1) gained, the protection that injection finishes in nitrogen drops to room temperature, obtains black liquor.
(4) black liquor obtains sediment under conditions of centrifugation rate is 4000rpm, the time is 120 seconds after centrifugation,
Mixed liquor of the sediment through n-hexane-ethanol washs 3 times, is passed through under conditions of temperature is 30 DEG C, vacuum is -0.09MPa
Constant weight is dried under vacuum to, produces Fe nano particles.
Wherein：
The mixed liquor of n-hexane-ethanol and the volume ratio of black liquor are 0.5 mL：1 mL.
The mixed liquor of n-hexane-ethanol refers to n-hexane and absolute ethyl alcohol by 2：1 volume ratio mixes.
Above-mentioned steps (1) ~ (3) the flow velocity of middle nitrogen be 30mL/min.
A kind of method that Fe nano particles are prepared using carbon quantum dot as crystal seed of embodiment 2, comprises the following steps：
(1) ferric acetyl acetonade is dissolved in oleyl amine solution, is stirred at room temperature and is passed through nitrogen 40min, then in nitrogen
Protection under with 20 DEG C/min speed be heated to 200 DEG C, and in being incubated 60min at this temperature, while quick at such a temperature
Inject tri octyl phosphine；Then temperature is raised to 250 DEG C, and in being incubated 60min at this temperature, obtains dark red liquid.
Wherein：The mass volume ratio of ferric acetyl acetonade and oleyl amine solution is 1.5mmol： 20mL；Ferric acetyl acetonade is pungent with three
The mass ratio of base phosphine is 1.5mmol：5.00mmol.
(2) citric acid is added in oleyl amine solution, adds octadecylene and be uniformly mixed, be stirred at room temperature and lead to
Enter nitrogen 40min, be then heated to 250 DEG C under the protection of nitrogen with 20 DEG C/min speed, and in being incubated at this temperature
100min, while tri octyl phosphine is rapidly injected at such a temperature；After insulation terminates, faint yellow clarified solution is obtained.
Wherein：The mass volume ratio of citric acid and oleyl amine solution is 0.1g：5mL；The quality volume of citric acid and octadecylene
Than for 0.1g：10mL；The mass ratio of citric acid and tri octyl phosphine is 0.1g： 5.00mmol.
(3) faint yellow clarified solution is continued to be warming up to 350 DEG C, and at this temperature using syringe pump with 10mL/h speed
The dark red liquid of implantation step (1) gained, the protection that injection finishes in nitrogen drop to room temperature, obtain black liquor.
(4) black liquor obtains sediment under conditions of centrifugation rate is 9000rpm, the time is 300 seconds after centrifugation,
Mixed liquor of the sediment through n-hexane-ethanol washs 9 times, is passed through under conditions of temperature is 60 DEG C, vacuum is -0.07MPa
Constant weight is dried under vacuum to, produces Fe nano particles.
Wherein：
The mixed liquor of n-hexane-ethanol and the volume ratio of black liquor are 3 mL：1 mL.
The mixed liquor of n-hexane-ethanol refers to n-hexane and absolute ethyl alcohol by 4：1 volume ratio mixes.
Above-mentioned steps (1) ~ (3) the flow velocity of middle nitrogen be 60mL/min.
A kind of method that Fe nano particles are prepared using carbon quantum dot as crystal seed of embodiment 3, comprises the following steps：
(1) ferric acetyl acetonade is dissolved in oleyl amine solution, is stirred at room temperature and is passed through nitrogen 30min, then in nitrogen
Protection under with 10 DEG C/min speed be heated to 130 DEG C, and in being incubated 30min at this temperature, while quick at such a temperature
Inject tri octyl phosphine；Then temperature is raised to 180 DEG C, and in being incubated 30min at this temperature, obtains dark red liquid.
Wherein：The mass volume ratio of ferric acetyl acetonade and oleyl amine solution is 0.5mmol：15mL；Ferric acetyl acetonade is pungent with three
The mass ratio of base phosphine is 0.5mmol：2.00mmol.
(2) citric acid is added in oleyl amine solution, adds octadecylene and be uniformly mixed, be stirred at room temperature and lead to
Enter nitrogen 30min, be then heated to 200 DEG C under the protection of nitrogen with 10 DEG C/min speed, and in being incubated at this temperature
50min, while tri octyl phosphine is rapidly injected at such a temperature；After insulation terminates, faint yellow clarified solution is obtained.
Wherein：The mass volume ratio of citric acid and oleyl amine solution is 0.05g：2mL；The quality volume of citric acid and octadecylene
Than for 0.05g：5mL；The mass ratio of citric acid and tri octyl phosphine is 0.05g：2.40mmol.
(3) faint yellow clarified solution is continued to be warming up to 315 DEG C, and at this temperature using syringe pump with 5mL/h speed note
Enter the dark red liquid of step (1) gained, the protection that injection finishes in nitrogen drops to room temperature, obtains black liquor.
(4) black liquor obtains sediment under conditions of centrifugation rate is 8000rpm, the time is 180 seconds after centrifugation,
Mixed liquor of the sediment through n-hexane-ethanol washs 7 times, is passed through under conditions of temperature is 30 DEG C, vacuum is -0.07MPa
Constant weight is dried under vacuum to, produces Fe nano particles.
Wherein：
The mixed liquor of n-hexane-ethanol and the volume ratio of black liquor are 0.5 mL：1 mL.
The mixed liquor of n-hexane-ethanol refers to n-hexane and absolute ethyl alcohol by 3：1 volume ratio mixes.
Above-mentioned steps (1) ~ (3) the flow velocity of middle nitrogen be 40mL/min.
A kind of method that Fe nano particles are prepared using carbon quantum dot as crystal seed of embodiment 4, comprises the following steps：
(1) ferric acetyl acetonade is dissolved in oleyl amine solution, is stirred at room temperature and is passed through nitrogen 20min, then in nitrogen
Protection under with 8 DEG C/min speed be heated to 150 DEG C, and in being incubated 20min, while quick note at such a temperature at this temperature
Enter tri octyl phosphine；Then temperature is raised to 170 DEG C, and in being incubated 20min at this temperature, obtains dark red liquid.
Wherein：The mass volume ratio of ferric acetyl acetonade and oleyl amine solution is 0.3mmol：10mL；Ferric acetyl acetonade is pungent with three
The mass ratio of base phosphine is 0.3mmol：1.50mmol.
(2) citric acid is added in oleyl amine solution, adds octadecylene and be uniformly mixed, be stirred at room temperature and lead to
Enter nitrogen 20min, be then heated to 170 DEG C under the protection of nitrogen with 8 DEG C/min speed, and in being incubated at this temperature
30min, while tri octyl phosphine is rapidly injected at such a temperature；After insulation terminates, faint yellow clarified solution is obtained.
Wherein：The mass volume ratio of citric acid and oleyl amine solution is 0.03g：1mL；The quality volume of citric acid and octadecylene
Than for 0.03g：3mL；The mass ratio of citric acid and tri octyl phosphine is 0.03g：1.50mmol.
(3) faint yellow clarified solution is continued to be warming up to 280 DEG C, and at this temperature using syringe pump with 3mL/h speed note
Enter the dark red liquid of step (1) gained, the protection that injection finishes in nitrogen drops to room temperature, obtains black liquor.
(4) black liquor obtains sediment under conditions of centrifugation rate is 6000rpm, the time is 180 seconds after centrifugation,
Mixed liquor of the sediment through n-hexane-ethanol washs 5 times, is passed through under conditions of temperature is 40 DEG C, vacuum is -0.08MPa
Constant weight is dried under vacuum to, produces Fe nano particles.
Wherein：
The mixed liquor of n-hexane-ethanol and the volume ratio of black liquor are 1.5 mL：1 mL.
The mixed liquor of n-hexane-ethanol refers to n-hexane and absolute ethyl alcohol by 2.5：1 volume ratio mixes.
Above-mentioned steps (1) ~ (3) the flow velocity of middle nitrogen be 50mL/min.
A kind of method that Fe nano particles are prepared using carbon quantum dot as crystal seed of embodiment 5, comprises the following steps：
(1) ferric acetyl acetonade is dissolved in oleyl amine solution, is stirred at room temperature and is passed through nitrogen 25min, then in nitrogen
Protection under with 15 DEG C/min speed be heated to 160 DEG C, and in being incubated 40min at this temperature, while quick at such a temperature
Inject tri octyl phosphine；Then temperature is raised to 200 DEG C, and in being incubated 40min at this temperature, obtains dark red liquid.
Wherein：The mass volume ratio of ferric acetyl acetonade and oleyl amine solution is 1mmol：10mL；Ferric acetyl acetonade and trioctylphosphine
The mass ratio of phosphine is 1mmol：3.50mmol.
(2) citric acid is added in oleyl amine solution, adds octadecylene and be uniformly mixed, be stirred at room temperature and lead to
Enter nitrogen 25min, be then heated to 210 DEG C under the protection of nitrogen with 15 DEG C/min speed, and in being incubated at this temperature
60min, while tri octyl phosphine is rapidly injected at such a temperature；After insulation terminates, faint yellow clarified solution is obtained.
Wherein：The mass volume ratio of citric acid and oleyl amine solution is 0.08g：3mL；The quality volume of citric acid and octadecylene
Than for 0.08g：7mL；The mass ratio of citric acid and tri octyl phosphine is 0.08g：3.20mmol.
(3) faint yellow clarified solution is continued to be warming up to 300 DEG C, and at this temperature using syringe pump with 5mL/h speed note
Enter the dark red liquid of step (1) gained, the protection that injection finishes in nitrogen drops to room temperature, obtains black liquor.
(4) black liquor obtains sediment under conditions of centrifugation rate is 7500rpm, the time is 240 seconds after centrifugation,
Mixed liquor of the sediment through n-hexane-ethanol washs 5 times, is passed through under conditions of temperature is 50 DEG C, vacuum is -0.08MPa
Constant weight is dried under vacuum to, produces Fe nano particles.
Wherein：
The mixed liquor of n-hexane-ethanol and the volume ratio of black liquor are 2 mL：1 mL.
The mixed liquor of n-hexane-ethanol refers to n-hexane and absolute ethyl alcohol by 3.5：1 volume ratio mixes.
Above-mentioned steps (1) ~ (3) the flow velocity of middle nitrogen be 35mL/min.
A kind of method that Fe nano particles are prepared using carbon quantum dot as crystal seed of embodiment 6, comprises the following steps：
(1) ferric acetyl acetonade is dissolved in oleyl amine solution, is stirred at room temperature and is passed through nitrogen 35min, then in nitrogen
Protection under with 10 DEG C/min speed be heated to 180 DEG C, and in being incubated 45min at this temperature, while quick at such a temperature
Inject tri octyl phosphine；Then temperature is raised to 230 DEG C, and in being incubated 45min at this temperature, obtains dark red liquid.
Wherein：The mass volume ratio of ferric acetyl acetonade and oleyl amine solution is 1.3mmol：15mL；Ferric acetyl acetonade is pungent with three
The mass ratio of base phosphine is 1.3mmol：4.00mmol.
(2) citric acid is added in oleyl amine solution, adds octadecylene and be uniformly mixed, be stirred at room temperature and lead to
Enter nitrogen 35min, be then heated to 230 DEG C under the protection of nitrogen with 10 DEG C/min speed, and in being incubated at this temperature
80min, while tri octyl phosphine is rapidly injected at such a temperature；After insulation terminates, faint yellow clarified solution is obtained.
Wherein：The mass volume ratio of citric acid and oleyl amine solution is 0.05g：3mL；The quality volume of citric acid and octadecylene
Than for 0.05g：8mL；The mass ratio of citric acid and tri octyl phosphine is 0.05g：4.40mmol.
(3) faint yellow clarified solution is continued to be warming up to 330 DEG C, and at this temperature using syringe pump with 8mL/h speed note
Enter the dark red liquid of step (1) gained, the protection that injection finishes in nitrogen drops to room temperature, obtains black liquor.
(4) black liquor obtains sediment under conditions of centrifugation rate is 8000rpm, the time is 240 seconds after centrifugation,
Mixed liquor of the sediment through n-hexane-ethanol washs 7 times, is passed through under conditions of temperature is 40 DEG C, vacuum is -0.09MPa
Constant weight is dried under vacuum to, produces Fe nano particles.
Wherein：
The mixed liquor of n-hexane-ethanol and the volume ratio of black liquor are 0.5 mL：1 mL.
The mixed liquor of n-hexane-ethanol refers to n-hexane and absolute ethyl alcohol by 3：1 volume ratio mixes.
Above-mentioned steps (1) ~ (3) the flow velocity of middle nitrogen be 45mL/min.
Claims (7)
1. a kind of method that Fe nano particles are prepared using carbon quantum dot as crystal seed, comprises the following steps：
(1) ferric acetyl acetonade is dissolved in oleyl amine solution, is stirred at room temperature and is passed through 10 ~ 40min of nitrogen, then in nitrogen
Protection under with 5 ~ 20 DEG C/min speed be heated to 100 ~ 200 DEG C, and in being incubated 10 ~ 60min at this temperature, while in the temperature
Tri octyl phosphine is rapidly injected under degree；Then temperature is raised to 150 ~ 250 DEG C, and in being incubated 10 ~ 60min at this temperature, obtained black
Red liquid；The mass volume ratio of the ferric acetyl acetonade and the oleyl amine solution is 0.1 ~ 1.5mmol：5~20mL；The second
The mass ratio of acyl acetone iron and the tri octyl phosphine is 0.1 ~ 1.5mmol：1.00~5.00mmol；
(2) citric acid is added in oleyl amine solution, adds octadecylene and be uniformly mixed, be stirred at room temperature and be passed through nitrogen
10 ~ 40min of gas, then it is heated to 150 ~ 250 DEG C under the protection of nitrogen with 5 ~ 20 DEG C/min speed, and in protecting at this temperature
20 ~ 100min of temperature, while tri octyl phosphine is rapidly injected at such a temperature；After insulation terminates, faint yellow clarified solution is obtained；The lemon
Lemon is sour and the mass volume ratio of the oleyl amine solution is 0.01 ~ 0.1g：0.5~5mL；The matter of the citric acid and the octadecylene
Amount volume ratio is 0.01 ~ 0.1g：1~10mL；The mass ratio of the citric acid and the tri octyl phosphine is 0.01 ~ 0.1g：1.00~
5.00mmol；
(3) the faint yellow clarified solution is continued to be warming up to 250 ~ 350 DEG C, and in injecting the step using syringe pump at this temperature
Suddenly (1) the dark red liquid of gained, the protection that injection finishes in nitrogen drop to room temperature, obtain black liquor；
(4) the black liquor obtains sediment after centrifugation, and mixed liquor of the sediment through n-hexane-ethanol washs 3 ~ 9 times,
It is vacuum dried to constant weight, produce Fe nano particles.
A kind of 2. method that Fe nano particles are prepared using carbon quantum dot as crystal seed as claimed in claim 1, it is characterised in that：Institute
State step (1) ~ (3) the flow velocity of middle nitrogen be 30 ~ 60mL/min.
A kind of 3. method that Fe nano particles are prepared using carbon quantum dot as crystal seed as claimed in claim 1, it is characterised in that：Institute
Stating step, (3) middle injection rate is 1 ~ 10mL/h.
A kind of 4. method that Fe nano particles are prepared using carbon quantum dot as crystal seed as claimed in claim 1, it is characterised in that：Institute
Stating step, (4) the volume ratio of the mixed liquor of middle n-hexane-ethanol and black liquor is 0.5 ~ 3 mL：1 mL.
A kind of 5. method that Fe nano particles are prepared using carbon quantum dot as crystal seed as claimed in claim 1, it is characterised in that：Institute
The mixed liquor for stating step (4) middle n-hexane-ethanol refers to n-hexane and absolute ethyl alcohol by 2 ~ 4：1 volume ratio mixes.
A kind of 6. method that Fe nano particles are prepared using carbon quantum dot as crystal seed as claimed in claim 1, it is characterised in that：Institute
The condition for stating step (4) middle centrifugation refers to that centrifugation rate is 4000 ~ 9000rpm, and the time is 120 ~ 300 seconds.
A kind of 7. method that Fe nano particles are prepared using carbon quantum dot as crystal seed as claimed in claim 1, it is characterised in that：Institute
In stating step (4) vacuum drying condition refer to temperature be 30 ~ 60 DEG C, vacuum be -0.09 ~ -0.07MPa.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101241788A (en) * | 2007-01-15 | 2008-08-13 | 中国科学院化学研究所 | Biological compatibility magnetic nano crystal for high dissolving and stable distribution in physiologicalbuffer liquid and its making method |
| CN101433965A (en) * | 2008-12-17 | 2009-05-20 | 厦门大学 | Method for preparing monodisperse nickel nanoparticle |
| CN101525159A (en) * | 2009-04-20 | 2009-09-09 | 中南大学 | Solvothermal preparation method of monodisperse Fe3O4 nano-particles |
| CN103192086A (en) * | 2012-01-10 | 2013-07-10 | 中国科学院宁波材料技术与工程研究所 | Preparation method for controllable duplex metal alloy nano particle |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6676729B2 (en) * | 2002-01-02 | 2004-01-13 | International Business Machines Corporation | Metal salt reduction to form alloy nanoparticles |
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2016
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101241788A (en) * | 2007-01-15 | 2008-08-13 | 中国科学院化学研究所 | Biological compatibility magnetic nano crystal for high dissolving and stable distribution in physiologicalbuffer liquid and its making method |
| CN101433965A (en) * | 2008-12-17 | 2009-05-20 | 厦门大学 | Method for preparing monodisperse nickel nanoparticle |
| CN101525159A (en) * | 2009-04-20 | 2009-09-09 | 中南大学 | Solvothermal preparation method of monodisperse Fe3O4 nano-particles |
| CN103192086A (en) * | 2012-01-10 | 2013-07-10 | 中国科学院宁波材料技术与工程研究所 | Preparation method for controllable duplex metal alloy nano particle |
Non-Patent Citations (1)
| Title |
|---|
| 磁性金属铁、镍纳米粒子及其复合结构的合成与研究;中国优秀硕士学位论文全文数据库工程科技Ⅰ辑;《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》;20150715(第7期);B020-30 * |
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